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Antiquities Display Pittsburgh Conference copists. SSP was founded in 1946 to help Your key to memorabilia the exchange of information and ideas Pittcon '94 is the 45th joint collaboration the numerous spectroscopy labo navigating the exhibit of two sponsoring societies: The Society between ratories and spectroscopists in the Pitts for Analytical Chemists of Pittsburgh burgh area. The newly formed group be of historically (SACP) and the Spectroscopy Society of gan holding monthly meetings because of Pittsburgh (SSP). Each group has a distin the overwhelming response and took an significant analytical guished history. active interest in the yearly meetings of SACP. instruments, According to the 1950 Pittsburgh Con| ference, "In view of the similarity of the equipment, and < S basic aims and interests of the individual memorabilia ο
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rganizers of Pittcon '94 have arranged the Antiquities Dis play Museum to afford confer ees the opportunity to observe their roots as analytical chemists. Believing that it is important to remember pioneering scien tists and entrepreneurs and their instru mentation, co-chairs Richard Obrycki and Andrew G. Sharkey and their antiquities committee members have arranged a spe cial exhibit of historically significant ana lytical instrumentation to be displayed at the left rear of Level 3 (42 level) in McCormick Place's East Hall. The museum occupies approximately 6500 ft2 and is divided into 14 areas (see floor plan on p. 217 A): Pittsburgh Confer ence memorabilia, thermal equipment, atomic spectroscopy, polarography, autoanalyzers, particle size/surface area/ pore size instruments, NMR, balances, X-ray spectrometers, mass spectrometers, chromatography, 1950s laboratory, sur face analyzers, and IR/UV-vis spectro scopies. An alphabetical listing of instru ments and equipment scheduled to be exhibited appears in the box on p. 221 A. 212 A
Penn-Sheraton Hotel welcomes Pittcon
SACP was organized in 1942 to allow analytical chemists to meet and discuss ideas and problems. The group organized thefirstannual Pittsburgh Analytical Sym posium in 1945, and a second one-day meeting was held the following year at Mellon Institute. After sponsoring a twoday program at the William Penn Hotel in 1948, SACP initiated an Exposition of Modern Laboratory Equipment in 1949. By thistime,the scope of the meetings had increased and the programs attracted conferees and speakers from throughout the country. Before 1946 the Cooperative Spectros copy Laboratory of the University of Pitts burgh coordinated the sponsoring of local meetings of interest to industrial spectros-
Analytical Chemistry, Vol. 66, No, 4, February 15, 1994
meetings of the two societies, it was thought that a combined conference would be to the mutual benefit of all analytical chemists and spectroscopists." This collaboration resulted in thefirstPittsburgh Conference on Analytical Chemistry and Applied Spectroscopy. This section of the museum traces the 8 origins and growth of the Pittsburgh Conference from its early days in Pittsburgh, PA; Cleveland, OH; and Atlantic City, NJ. Thermal equipment
Thermal analysis refers to a group of techniques that measure changes such as weight loss and dimension in a material as
DuPont Model 900 thermal analyzer (1962) 0003 - 2700/94/0366 -212A/$04.50/0 © 1994 American Chemical Society
Museum Guide it is heated or cooled. These techniques can be used to characterize a wide spec trum of materials, including pharmaceuti cals, inorganic materials, foods, and petro leum products. Most often the techniques are used to evaluate polymers and provide information about properties such as the glass transition temperature, melting point, and degrees of crystallinity. Two instruments will be displayed: the Model 900 thermal analyzer, contributed by TA Instruments, and the DSC 1 differential scanning calorimeter, contributed by Per kin Elmer. The Model 900 thermal analyzer was introduced by TA Instruments, which was then a business unit within DuPont, in 1962. The first industrial-grade thermal analyzer, it allowed analysts to measure weight changes of materials upon heating and the heats and temperatures of transi tions and reactions. More than 50,000 in struments were sold. Perkin Elmer introduced the DSC 1 differential scanning calorimeter at the 1963 Pittsburgh Conference. This instru ment applied modern electronic and me chanical technology to thermal analysis and was the first in a family of instruments that included differential thermal analyz ers, differential mechanical analyzers, and differential scanning calorimeters. More than 3000 instruments were produced from 1963 to 1978. Atomic spectroscopy
Instruments and equipment on display include the Jarrell Ash 21-ft. Wadsworth spectrograph (contributed by Thermo Jarrell Ash), gratings (contributed by Hi tachi), photomultiplier tubes (contributed by Hamamatsu), the original stand from
PRODUCTION CONTROL Q U A N T O M E T E R DIRECT R E A D I N G
ANALYSIS
Applied Research Laboratories No. 7200 production control quantometer (1950)
the first ARLICP-AES instrument and the ARL production control quantometer (PCQ) (contributed by Fisons Instru ments), Model 303 AA spectrophotometer (contributed by Perkin Elmer), a 3-m grat ing spectrograph (contributed by Baird Analytical), and two early AA precursor instruments loaned by Alan Walsh of CSIRO (Australia). Manufactured in 1943, the Jarrell Ash 21-ft. Wadsworth stigmatic grating spec trograph incorporates a 6-in.-diameter, 21-ft., 10-in. radius of curvature concave grating as a dispersing element. R. W. Wood and Wilbur Perry at the Johns Hop kins University ruled the grating with 15,000 grooves/in. Two 4- χ 10-in. plates covered 5000 Â at 5 A/mm in the first order or 2500 Â at 2.5 A/mm in the second order. The largest and most expensive spectrograph available at the time, it was widely used to identify and measure uranium in mineral samples as well as trace and alloying elements in hightemperature superalloys for aircraft en-
gines. Approximately 60 instruments were sold worldwide. Hitachi has loaned six gratings developed from 1976 to 1987. On display are a tripartite stigmatic ruled concave grating (50 χ 40 χ 10 mm) for a fluorescence spec trophotometer, an aberration-corrected ruled concave grating (20 χ 13 χ 10 mm) for a flat-field normal incidence UV-vis spectrograph, a double-blaze ruled plane grating (68.5 χ 68.5 χ 10 mm) for an IR spectrophotometer, an aberration-cor rected ruled concave grating (30 χ 30 χ 10 mm) for a flat-field grazing incidence soft X-ray spectrograph, a large ruled plane grating (150 χ 150 χ 30 mm) for a large spectrograph, and a variable-linespacing ruled plane grating (200 χ 80 χ 30 mm) for a spectrometer to explore the extreme UV wavelength region. Hamamatsu has sent side window pho tomultiplier tubes used in spectrophotom eters. The R108 series, introduced in 1961, is compact and features a quartz envelope. The R136 series (1965) offered a red-enhanced response. The R300, R306, and R427 series (1969) were 0.5-in.-diameter tubes for direct-reading emission spec trophotometers. The R446 series, intro duced in 1970, was a multi-alkali, opaque photocathode; the R928 series introduced in 1975 was a red-enhanced, opaque pho tocathode. Fisons Instruments has provided the original stand used to house the induc tively coupled plasma from the first Ap plied Research Laboratories (ARL) ICPAES instrument. ARL, now part of Fisons Instruments, launched its first commercial ICP instrument in 1974. These early in struments were used for glass and geol ogy applications.
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GUIDE The ARL No. 7200 PCQ was launched in 1950 in response to industry's demand for a relatively low-priced instrument that would permit rapid direct-reading analy sis. The novel spectrometer design fea tured a vertical arrangement of the Row land circle, which was 1.5 m in diameter, and reduced the required footprint of the instrument. Maximum flexibility was achieved by having a phototube for each spectrum line of interest and a set of con trols for every concentration range of in terest. Thus, one instrument could be used to analyze low alloy steels, pig iron, and slags; low alloy, stainless, and tool steels; aluminum and magnesium alloys; and brasses and bearing alloys. Perkin Elmer's Model 303 AA spectro photometer, introduced in 1963, was the first double-beam AA spectrophotometer produced in large quantities. Results could be read directly in percent absorp tion on a precise three-digit counter or, by using an accessory, the instrument pro vided direct concentration readings in the desired units on a four-digit illuminated display. Over the next 20 years, more than 20,000 instruments were produced. The Baird Corporation manufactured the first commercially available 3-m grat ing spectrograph in 1936 and continued production through the early 1970s. By using a diffraction grating rather than a prism as the dispersing device, it was pos sible to design an instrument that was more optically efficient than other spectro graphs of thetime.The spectrograph was mounted on a rugged steel frame, and electrically operated controls that moved the grating photographic plates were lo cated on the front panel. The instrument displayed here, donated by Stanley Gedansky of Uniroyal Chemical Com pany, was purchased in 1940 by the U.S. Rubber Company. Its useful lifetime spanned the period from 1940 through 1989, during which more than 9000 photo graphic plates were exposed and up to 20 samples per plate were analyzed.
the 1982 Pittsburgh Conference in Atlan tic City. Since then, more than 2000 ro botic systems have been installed. ζ LU
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Princeton Applied Research Model 197 polarographic analyzer (1971)
larography, pulse polarography, differen tial pulse polarography, linear sweep voltammetry at a stationary electrode, and anodic stripping analysis. The instrument was supplied with a droptimerthat pre cisely dislodged the mercury drop after a preselected period. This model, designed for use in teaching electrochemistry in a university setting, was also useful for the determination of trace and ultra trace lev els of heavy metals. Approximately 2340 polarographs (both the Model 174 and the upgraded Model 174A) were sold be tween 1971 and 1979. Autoanalyzers
In the early 1980s, analytical measure ments had improved dramatically and computer technology for data analysis was emerging. Sample preparation remained a labor intensive and sometimes trouble some step in analysis. Zymark developed its laboratory automation system (robot) surrounded by manual stations that per formed individual sample preparation steps. A microprocessor-based controller managed the robot, work flow, and mod ules to allow unattended and automated analysis. The robot and controller on dis play are the actual system introduced at
Polarography
Model 174 polarographic analyzer, loaned by Princeton Applied Research/EG&G, was offered for sale on October 1,1971. It was thefirstall-electronic, solid-state po larographic instrument that could be used to perform normal and sampled dc po-
Particle size/surface area/pore size instruments
Micromeritics DigiSorb 2500 surface area analyzer (1972)
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Analytical Chemistry, Vol. 66, No. 4, February 15, 1994
The Coulter Model A instrument revo lutionized the counting and sizing of blood cells and microscopic particles. In the clinical laboratory, it replaced micro scopes for counting and provided quick and accurate blood counts to physicians dealing with emergency situations. In the industrial laboratory, it replaced sieving and other manual sizing methods and pro vided increased speed and resolution. The unit displayed here is serial no. 13. The Numinco Orr surface analyzer, first produced in 1968, was one of the first commercially available nonglass instru ments for measuring the surface area, pore volume, and pore distribution of solid materials. Scientists no longer had to be come experts in glass blowing before they could determine the surface area, pore volume, and pore volume distributions of powders being studied. Experimenters
According to James Shoolery, who helped develop the A-60, the most difficult technical challenge encountered was lock ing the frequency of the magnetic field. This problem was solved by irradiating a small amount of water in the probe near the sample at 60 MHz and modulating the signal with an audio frequency generated by closing a loop to create a nuclear side band oscillator. The audio circuit oscil lated only at a frequency that put the side band exactly at the water resonance line frequency. The A-60 was well received in the mar ketplace, both by analytical chemists and by chemists involved in synthesis and nat ural products applications. Over its life time, more than 1000 spectrometers were sold, 120 of these in the first year.
were able to compare results from a larger number of samples as well as between samples with a high degree of accuracy. More than 500 units were sold. The SediGraph 5000 automatic particle analyzer was introduced in 1969 and was one of the steps toward automatic particle size analysis. The instrument required less manual manipulation and time than did other particle sizing techniques; thus, more samples could be analyzed and re sults from different laboratories could be compared with reduced operator bias. Worldwide, more than 1500 analyzers were sold. The DigiSorb 2500 surface area ana lyzer that was produced in 1972 was one of the first pieces of commercially avail able laboratory equipment controlled by a digital computer. It increased the accu racy and reproducibility of surface adsorp tion measurements and substantially re duced the operator time required for analysis. Computer control of instrument operation, data acquisition, and reporting allowed virtually unattended operation around the clock.
Balances Balances on display include the Harvard trip balance, contributed by Ohaus Corpo ration; the assayer's balance, Type Τ analyt ical balance, Type BB analytical balance, and Model FDM microbalance—all of
NMR PPG Industries has loaned a Varian A-60 NMR spectrometer, which was sold as an affordable proton spectrometer that of fered high stability and sensitivity. De signed by Varian Associates with a 6-in. electromagnet operating at 60 MHz to provide resolution equal to that of the pre decessor HR-60 spectrometer, which had a 12-in. electromagnet, the instrument was fashioned in a console style that would fit into the laboratory. It included a cabinet for the electronics, a control panel, and a flatbed recorder to produce the NMR spectrum on precalibrated chart paper.
Ainsworth assayer's balance (ca. 1888)
which were manufactured by William Ainsworth & Sons and loaned by its succes sor, the Denver Instrument Company; the B5 analytical balance, sent by Mettler To ledo; and the Cahn Model M-10 microbal ance, contributed by Orion Research. to ζ Introduced in 1910, the Ohaus Harvard Ω UJ trip balance was designed for use in labo u. Ο >σι ratories, industry, and schools. In the mid19308, Gustav Ohaus received a patent for Ο Ο the self-aligning bearings used on this balance, which create less friction and last Œ LU ¥ Ο LU
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Varian A -60 NMR spectrometer (1961)
longer because of reduced wear. This bal ance is still manufactured by Ohaus. The oldest of the William Ainsworth balances is the assayer's balance, which was first manufactured in 1879. The first American-made balance, it offered a capac ity of 2 g and a resolution of 0.03 mg. The Type Τ analytical balance (1932) was the first short-beam analytical balance. With a capacity of 200 g and a resolution of 0.4 mg, it provided quick analytical response. The Type BB analytical balance was a directreading chain-type balance that eliminated tedious calculations. First manufactured in 1940, it had a capacity of 200 g, and its reso lution was 0.2 mg. The fourth unit, the Model FDM microbalance, was manufac tured in 1942 and was the first Americanmade microbalance. It offered a capacity of 20 g and a resolution of 1 μg. The Mettler B5 analytical balance was invented in 1945 and sold commercially beginning in 1947. Developed by Erhard Mettler in Switzerland, it was the first sin gle-pan precision weighing device; it had a capacity of 200 g and a readability of 0.05 g. It used the substitution principle, which meant that built-in mechanically lifted weights could be dialed in as needed. Worldwide, more than 50,000 B5 balances were sold between 1947 and 1974. In the United States, more than 10,000 were sold between 1955 and 1974. The Cahn Model M-10 microbalance from Orion Research was the first envi ronment-insensitive microbalance and the first commercial instrument to use an am meter coil as the sensing element. X-ray spectrometers Instruments on display include the Model 1800 Portaspec portable X-ray spectro graph, contributed by Cianflone Scientific Instruments; EDAX Model 707 analyzer and EDAX carbon, oxygen, and nitrogen (ECON) detector, sent by EDAX Interna tional; Norelco powder diffractometer, contributed by Philips Electronic Instru ments; and JCPDS search/match cards, loaned by ICDD. The Model 1800 instrument was intro duced in 1969. It was the first portable wavelength-dispersive XRF spectrograph that allowed analytical capabilities to be moved from the laboratory to the job site. EDAX Model 707 analyzer, introduced in 1971, was the first energy-dispersive
Analytical Chemistry, Vol. 66, No. 4, February 15, 1994 215 A
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EDAX Model 707 analyzer (1971)
X-ray system to use a microprocessor. This factor revolutionized data collection and display capability, enabled automatic identification, and was the basis of quantitative microanalysis by energy-dispersive X-ray spectroscopy (EDS). The system also featured a parallel interface to a 4 KB Data General computer with teletype I/O. More than 1000 units were sold throughout the world. The ECON detector was thefirstwindowless EDS detector. This detector allowed analysts to determine elements down to carbon by EDS. Several thousand units have been sold since the 1974 introduction. The Philips Model 2 powder diffractometer on display (serial no. 2) features a goniometer design pioneered by William Parrish and co-workers. It allowed the use of an electronic detector system that provided intensity and accuracy improvements over existing powder diffraction cameras. The improvements in convenience and accuracy spurred the development and acceptance of quantitative X-ray analysis. Phillips estimated that more than 15,000 diffractometers based on this X-ray optical design are still in operation today. JCPDS search/match cards from the 1940s will be displayed together with an exhibit of the advances in search/match routines through the years. Mass spectrometers
This section of the display museum will feature three posters, contributed by Mike Grayson of the American Society for Mass Spectrometers (ASMS), and the HP 216 A
5992 GC/MS, contributed by Hewlett Packard. Thefirstposter traces the origins of ASMS from the meetings of users of CEC 103 mass spectrometers to the present day. The program of the first meeting of ASMS, held in conjunction with the Pittsburgh Conference on Analytical Chemistry and Applied Spectroscopy in March 1953, is reproduced. The second poster depicts the history of the MS-9 mass spectrometer, the first commercially available double-focusing instrument equipped with electrical detection. Based on a design concept developed by Professor Al Nier at the University of Minnesota, it revolutionized accurate mass measurement techniques for organic applications. A variety of models were developed and marketed by Metropolitan Vickers/Associated Electrical Industries/Kratos over the 25-year life of the instrument.
GC/Mass Spectrometer Data Systems
HP 5992 GC/MS instrument
The third poster recounts the history of the Model 103 C mass spectrometer. The Consolidated Engineering Corporation introduced a single-focusing mass spectrometer in the late 1940s that was the predecessor to the Model 103 series of instruments. These mass spectrometers were legendary in the petrochemical industry from the time of their introduction to the last decade. These instruments were used to develop important analytical methods for analyzing process streams in hours instead of days. Consequently, pilot plant development proceeded at a more rapid and economical pace. In the period from 1943 to 1965, more than 200 units were sold. Model 5992 GC/MS instrument is a
Analytical Chemistry, Vol. 66, No. 4, February 15, 1994
digitally controlled system in which computer control of the mass spectrometer settings replaces knobs and dials. Computer control also made it possible to introduce automatic tuning and to reduce cost and footprint size. Commonly known as a benchtop GC/MS instrument, the system included a hyperbolic quadrupole to provide sharp, consistent peak shapes and to increase system sensitivity. Chromatography
This section of the display museum is divided into three sections: gas chromatographs, liquid chromatographs, and supercritical fluid chromatographs. Gas chromatographs. The Carlo Erba Fractovap Model GI (1968) was designed to be a cost-effective, easy-to-use singlecolumn gas chromatograph for use in quality control laboratories. Loaned by Fisons Instruments, it was thefirstinstrument to use a vertical design for both the injector and the detector, thereby providing a total absence of dead volume in the system. It was also the instrument used to produce the first splitless injection system in which the sample was condensed at the top of the column and released by rapid temperature programming. Hewlett Packard's Instrument Division was known as the F&M Scientific Corporation before its acquisition by HP in 1965. In late 1972, HP also acquired the German Hupe-Busch Co. The Instrument Division has contributedfiveGC instruments to the GC portion of the chromatography museum. F&M Scientific Model 700 GC, which was introduced around 1961, was an improved version of the gas chromatograph that F&M introduced at the 1959 Pittsburgh Conference. Offering linear temperature programming and independent control of oven (column) and detector temperatures, it was equipped with a thermal conductivity detector. Later options included flame ionization, electron capture, and micro cross-section detectors. F&M Scientific Model 720 GC made its debut in 1962 as thefirstinstrument to offer linear temperature programming, dual-column baseline compensation, and a thermal conductivity detector. F&M Scientific Model 810 GC was available in the early 1960s. Designed as the state-of-the-art instrument of its time,
Thermal Equipment
it incorporated linear temperature pro gramming, dual-column baseline compen sation, thermal conductivity or flame ion ization detectors, and a variety of accessories such as injection and effluent splitters and collection systems. F&M Scientific Model 402 biomedical GC debuted in the mid-1960s as an instrument designed specifically for the medical-biochemical field. The design incorporated a floor-standing oven to ac commodate vertical U-shaped glass col umns. Features included an on-column injection system; dual effluent splitters; and the option of simultaneously installing flame ionization, ion emission, and elec tron capture micro cross-section or microcoulometric detectors. In the mid-1960s, glass open-tubular (capillary) columns began to be used in GC. These columns were generally made by chromatographers, who drew them from regular 4-mm-i.d. glass tubing to cap illary dimensions using instruments such as the Hupe and Busch Model 1045 glass drawing machine (1966). The Pye Argon gas chromatograph (1958), contributed by Orion Research, was introduced at the Second Interna tional Symposium on GC in Amsterdam, The Netherlands. It was the first gas chro matograph equipped with the argon ion ization detector invented by J. E. Love lock. A floor-standing unit for use with packed columns and in isothermal opera tion, it had a significant impact, primarily in Europe, on the evolution of GC. Model 154 vapor fractometer, intro duced in 1955 by Perkin Elmer, was the first commercial gas chromatograph. It employed a highly sensitive thermistor detector and easy-to-use U-shaped col umns that contained both absorption- and partition-type packings.
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Perkin Elmer Model 154 vapor fractometer (1955)
EXIT Perkin Elmer's Atomic Model 800 gas chro Pittsburgh Spectroscopy Conference matograph (1962) was Memorabilia the first dual-column baseline compensation unit with linear tempera NMR Polarography ture programming, a AutoanalyzersX-ray differential flame ioniza Spectrometers Balances Particle Size/ tion detector, and 1/8Surface Area/ Pore Size in.-o.d. columns as stan Instruments Mass dards. Later, a dual Surface Spectrometers Analyzers thermal conductivity 1950s detector was added to Lab the system. Perkin Elmer Model Chromatography 226 gas chromatograph IR/UV-vis (1966) was specifically ENTRANCE designed for open-tubu lar columns, but it could also be used with smallFloor plan of the Antiquities Display Museum, located at the left rear of Level 3 in McCormick Place's East Hall diameter (1/8 in.), thinwalled, short packed columns. Offered with linear temperature pany was acquired by Varian in the spring programming, a linear split system, and a of 1966, and the two chromatographs de flame ionization detector, the instrument's scribed below were contributed by Varian. unique feature was its method of column Aerograph Model A-90 gas chromato heating. The stainless-steel capillary or graph (1957) was the first instrument packed columns were coiled into a flat produced by Wilkens Instrument & Re spiral that was pressed together with a search, Inc. It was a small, unsophisti heated plate (like a pancake), permitting cated machine that offered a thermal con accurate following of the set temperature ductivity detector and isothermal oven program. control. Tremetrics, the successor of MicroAerograph Model 600 D HyFi gas Tek and Tracor, two companies involved chromatograph (1961) was equipped with in the early development of GC, has con a flame ionization detector (the name tributed two instruments to the display. HyFi derives from ^drogen/lame ioniza Micro-Tek Model 222 gas chromatograph tion) and permitted ballistic temperature was designed as a floor-standing unit pri programming. Later versions included an marily for the biochemical market. It had optional electron capture detector. The four-column capability and could operate Model 600 displayed here is from 1964. simultaneously up to four detectors, Liquid chromatographs. Ion chroma among them the electron capture detector tography is used to separate, detect, and with 63Ni foil. This instrument has an allquantitate ionic species in solution in ap glass system with U-shaped glass columns. plications such as quality assurance, qual Tracor Model 321 Coulsen conductiv ity control, biotechnology, energy produc ity detector (1968) was one of the earliest tion, and environmental analysis and commercial electrolytic conductivity de control. The Dionex Model 10 ion chro tectors, which have become extremely matograph, which was introduced in the important in the pollution control field. fall of 1975, pioneered the technique of The special feature of the detector was the ion chromatography for the analysis of unique gas-liquid contact section of the inorganic anions and cations as the first glass conductivity cell. commercial instrument based on ion sepa ration technology, chemical eluent sup The present Chromatography Division of Varian began on Dec. 14,1956, as Wilk- pression, and conductivity detection. ens Instrument & Research, Inc., and its The Hupe and Busch 1010 A/B liquid gas chromatographs were marketed un chromatograph, loaned by Hewlett Pack der the trade name Aerograph. The cornard, was introduced in 1971 as one of the
Analytical Chemistry, Vol. 66, No. 4, February 15, 1994
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Waters Associates Model 401 refractometer (1959)
first commercial liquid chromatographs. It used a unique reciprocating piston-dia phragm pumping system. Isco has provided two pieces of equip ment for this section of the museum. Model U LC UV detector (1961) was the first commercial UV detector to produce chromatograms in linear absorbance (op tical density). It represented the first slope-sensing peak detector, called "auto matic index" at the time. This electronic trigger for peaking beginning and ending points was later used in computing inte grators. Other features included a built-in chart recorder and a remote 254-nm opti cal unit with interchangeable flow cells. The Dialagrad gradient pump for LC (1966) was thefirstprogrammable dualpump LC solvent delivery system to form gradients by varying the speed of each pump while maintaining constant total flow. It produced compositional gradients of up to 10 linear segments, with flow rate, gradient duration, and final composition set via dials. Stepper motors and rapid refill were new LC pump design concepts. Approximately 220 units were sold, and the dual-pump gradient patent was li censed to Waters, Varian, and other man ufacturers. Varian Aerograph Model 4010-01 liq uid chromatograph (1967) is one of the first commercial modern LC instruments. Varian began to investigate the possibility of LC instrumentation in 1966 by forming an LC R&D group. Itsfirstproduct, intro duced in 1967, was the 4000 series pres sure displacement pump. The unit dis played here is a version of that product, which incorporates afixed-wavelengthUV detector. Millipore Waters Chromatography Division, the successor of Waters Associ 218 A
when it was introduced. Prior to that time, ates, has madefivepieces of equipment researchers investigating this technique available for display. Waters Model 401 had to build their own equipment. refractometer (1959) was used by early researchers in LC to measure changes in the refractive index of sample constituents 1950s Laboratory and to correlate them with concentration. This portion of the display museum at Waters GPC Model 100 (1963) is a gel tempts to recreate the flavor of a vintage permeation chromatograph designed to laboratory of the 1950s. analyze polymers at elevated tempera The Model Β blender (1937) contrib tures. It is one of the first commercial liq uted by Waring Products Division is one uid chromatographs. in a line of blenders that have been used Waters Model 6000 pump (1971) is the for more than 50 years in laboratories for first pumping system designed specifically genetics, biomedical, and everyday labora tory applications. for LC. Featuring pulse-free flow without pulse dampeners, it permitted accurate compositional mixing of mobile phases. Before the introduction of the Waters Model U6K injector (1973), septum injec tors represented the state of the art in LC. Waters Pico-Tag amino acid analysis sys tem (1984) was thefirstprecolumn derivatization system designed exclusively for amino acid analysis. Supercriticalfluidchromatographs. The Lee Scientific Model 501 supercritical fluid chromatograph, provided by Dionex, first appeared at Pittcon in March 1986. ThefirstSFC system to use both openGeneral analytical lab at Standard Oil tubular and packed columns, it offered Company in Whiting, IN (1959) users the solubility of HPLC coupled with the important and universal flame ioniza tion detection mechanism of GC. The The Beckman Model G pH meter availability of capillary columns increased (1935), contributed by Beckman Instru the efficiency of SFC and the range of ana- ments, was Arnold Beckman's pioneer lytes that could be determined. product. The prototype instrument was developed in 1934 for a friend who was Hewlett Packard's Model 1082 (1982) unable to determine the pH of lemon juice was thefirstcommercial supercritical treated with S02 using traditional indica fluid chromatograph on the market. Al though lacking several features present in tor methods. The constant use of the re sulting "acidimeter" prompted Beckman second-generation instruments, it pro to start National Technical Laboratories to vided a new advance in the technology manufacture and market the pH meters. This company was later renamed Beck man Instruments. In addition to the Model G pH meter, Beckman Instruments has also loaned a Model Β spectrophotometer for display. Prior to the introduction of the Model 801 digital pH meter in 1965, all pH me ters were analog or used rotary wheels for .'-'.'. digital display. This meter, contributed by Orion Research, was thefirsttrue digital CAPILLARY meter that used l-in.-high neon segments; SUPERCRITICAL FLUID advertisements promised it "could be CHROMATOGRAPHY.* read from 30 ft. away." Several thousand pH meters were sold over the lifetime of Lee Scientific Model 501 supercritical fluid the Model 801. chromatograph (1986)
Analytical Chemistry, Vol. 66, No. 4, February 15, 1994
The fluoride ion-selective electrode, Can, the film is used to seal beakers, introduced commercially in 1966 and con flasks, test tubes, and petri dishes. tributed by Orion Research, is widely Additional instruments and equipment used and accepted today; according to its scheduled for display include a Buchler manufacturer, it is the single most impor rotoevaporator (courtesy of Labconco), a tant ion-selective electrode. The electrode Fisher electrophotometerfiltercolorime displayed is the first experimental model ter (contributed by Fisher Scientific), and made with a laser crystal and held to carbon electrodes from Ultra Carbon gether with black sealing wax. (loaned by Carbone of America). Gordon Publications has contributed Analytical Chemistry has assembled a the framed original front page of the first retrospective exhibit that focuses on the issue of Laboratory Equipment, which be people, events, and scientific advances gan publication in 1963 and introduced that have contributed to the evolution of new products and services to analytical measurement science, the development of chemists. the journal, and the growth of Pittcon over Kipp and Zonen has contributed a Kipp the past 45 years. hydrogen gas generator (1830). Designed by a Dutch pharmacist-chemist, the gen Surface analyzers erator was developed to produce hydro Instruments on display in this section of gen gas in a controlled manner in labora the museum include the HP 5950 X-ray tories via the reaction of Zn with H2S04. photoelectron spectrometer (contributed The heating mantle contributed by by the University of Pittsburgh), the 3M Glas-Col was invented by that company's . Model 520 ion scattering spectrometer founder, Glen Morey, who had been in and the 3M Combined ISS/SIM System jured in a laboratory fire that was started (contributed by Advanced R&D), and the by an open flame. Deciding that it was Physical Electronics Industries Model essential to develop a new method for 10-150 Auger Analyzer (contributed by heating flasks that would reduce this haz Perkin Elmer). ard, he invented the now familiar heating mantle. Various pH meters, glass, and hot plates have been contributed by Corning. Notable products include the first triplepurpose pH glass, which allowed readings over the full 0-14 pH range; digital pH meters; Model 135 meter with membrane switches; and thefirstglass-ceramic top hot plate, which was introduced in 1964. Eberbach has loaned two items: Cata log # 1250 ultraspeed electroanalyzer for high-speed determination of copper and Hewlett Packard 5950 X-ray spectrometer lead by the electrodeposition process and Catalog # 1510 Dyna-Cath, which sepa rates metals by the mercury cathode The HP 5950 X-ray photoelectron spec technique. trometer dates from the early 1970s and Brinkmann Instruments has sent the includes vacuum equipment, an X-ray Metrohm Titrator Model 336, which was monochromator, a hemispherical electro introduced in 1958. The company's first static analyzer, and an inlet system. This generation of automatictitrators,the in instrument is noteworthy for several rea strument featured a piston buret and sons: It was the first monochromatic XPS could plot pH or mV versus volume of instrument, it was the only XPS instru titrant and afirstderivative. ment built by HP, and it became the model for the small-spot XPS instrument Parafilm M self-sealing thermoplastic, from Surface Science Labs. Approximately introduced in 1934 and virtually un changed today, was probably as familiar to 50 instruments were sold. This instant commercial success helped pave the way working chemists in the 1950s as it is for the future development of XPS. now. Contributed by American National
The Model 520 ion scattering spec trometer (1969), contributed by Advanced R&D, is a 90° sector instrument with vac uum chamber, cabinetry, and electronics. It used one small 25 L/s ion pump with Ti sublimators and a 1-mm ion beam gun, and had no sample vacuum introduction system or data system. The unit on dis play was one of thefirstsector ion scatter ing spectrometers manufactured by 3M and was used extensively for trade shows and sales demonstrations. The 3M combined ion scattering spectrometry/secondary ion mass spectrome try system with an updated cylindrical mirror analyzer ISS system was contrib uted by Advanced R&D and manufactured from 1976 to 1981. It includes a UTI quadrupole mass spectrometer, a sample intro duction system, a hard-wired Tracer Northern multiple-channel analyzer as a data system, the newly invented 125-μηι ion beam gun, electronic rank, and a newly designed low-current, ion-induced sample current imaging system. The sys tem shown here was one of the very first quadrupole SIMS systems commercially developed and sold by 3M. Model 10-150 cylinder mirror analyzer for Auger spectroscopy is contributed by Perkin Elmer. Manufactured by Physical Electronics Industries in 1972, this spec trometer was the first one designed for routine surface and thin-film elemental analysis for features smaller than 25 μπι. The analyzer was incorporated into the PHI Model 540 Auger electron spectrome ter, which was essential to the develop ment of silicon-based electronics. IR/UV-vis spectroscopies
Beckman Instruments contributed two instruments to this section of the mu seum: the Model IR-1 infrared spectropho tometer and the Model DU UV-vis spec trophotometer, as well as a selection of cells and sampling accessories. The Model IR-1 infrared spectrophotometer (1942) was a single-beam instrument that initially dispersed radiation with rock salt and quartz prisms. The instrument line resulted from a request made by the U.S. government for an instrument that would support research for the synthetic rubber program, which relied on butadiene, whose chemicalfingerprintwas detect able in the IR region. About 75 spectro-
Analytical Chemistry, Vol. 66, No. 4, February 15, 1994 219 A
£/££/ photometers were delivered between 1942 and 1945. With the advent of the Model DU UVvis spectrophotometer in 1941, the con cept of benchtop scientific instrumenta tion for every laboratory was born. Along with it came the beginnings of the com mercial scientific instrumentation indus try. The instrument wasfirstused to mea sure vitamins A and D in cod liver oil; it reduced a biological assay that took days and had an uncertainty of 25% to a deter mination that required minutes and pro vided an accuracy better than 1%. More than 21,000 DUs were sold before the product line was superseded in 1964. Milton Roy has provided two familiar instruments to the museum: the Bausch & Lomb Spectronic 20 and the AminoBowman spectrofluorometer. Since its introduction in 1954 as thefirstlow-cost grating instrument, the Spectronic 20 has enjoyed enormous success, and most chemists have used this instrument some time in their careers. Approximately 400,000 units have been placed around the world in all types of industrial, educa tional, and clinical laboratories. The Aminco-Bowman spectrofluorom eter, produced in the mid-1950s, was the first commercially available scanning fluorometer. Also on display will be the elec tronics subsystem for an early SLM 4800, thefirstcommercially successful phasemodulation lifetime spectrofluorometer. Graseby Specac has contributed three items of interest to this section of the mu seum. The F-04 cell was manufactured by Research Industrial Instrument Company (England) in 1954 for the Perkin Elmer
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Harrick Scientific's prism liquid cell 220 A
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Infracord instruments. The liquid sam pling cell, which was constructed of stain less steel, had a clip-type mount. Between 5000 and 6000 were sold over its lifetime. The 7000 variable cell, another liquid IR cell still in production, has a pathlength that can be varied to a maximum of 6 mm. Also on display is a catalog of IR and UV sampling accessories, including samplehandling and preparation accessories for solids, liquids, and gases, as well as a cell window polishing kit. G. L Carlson of GPU Nuclear Corp., a past president of the Pittsburgh Confer ence, has contributed an Evelyn photo electric colorimeter (macro model) from his personal collection. Manufactured by Rubicon and introduced around 1950, the single-cell, direct-reading photoelectric photometer was equipped with a light fil ter. It featured 18 narrow-band, all-glass filters covering the range from 375 to 765 μηι. The Rubicon Spotlight galvanom eter had a sensitivity of 0.8 μΑ full scale. The basic instrument, mounted in a wal nut case, sold for $380 in 1951. Harrick Scientific's exhibit is designed to provide historical insight into the devel opment of internal reflection spectros copy. It features Internal Reflection Spec troscopy, N. J. Harrick's landmark textbook that remains an important refer ence and educational tool for this power ful spectroscopic technique; frustrated reflectionfingerprinting,an early applica tion of the technique; and the prism liquid cell, one of thefirstcells developed for studies of aqueous solutions. Perkin Elmer provided the Model 12 single-beam IR spectrophotometer, the Model 21 IR spectrophotometer, and the Model 137 Infracord IR spectrophotome ter displayed here, as well as an exhibit of NaCl plates, demountable cells, and a KBr die. The Model 12 was one of the first commercially available IR spectrophotom eters and was introduced in 1944. It used a building block construction and evolved into the Models 12B and 12C in a short period of time; Model 12C was built as a modular system. The result of this evolu tionary process was the Model 13, intro duced in 1951 as the first double-beam IR spectrophotometer on the market. The success of the Model 21 greatly enhanced the reputation of Perkin Elmer. The energy flow in this double-beam in-
Analytical Chemistry, Vol. 66, No. 4, February 15, 1994
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Science Spectrum's Differential I light-scattering photometer (1970)
strument wasrightto left, exactly the op posite of the arrangement in the Model 12. According to Paul Wilks, this change was designed to improve the ease with which the slits could be aligned. More than 1000 were produced. The Model 137 IR spectrophotometer, which made its debut in 1959, was the first low-cost unit that offered a good price-to-performance ratio and was practi cal to use. As early as 1962, these instru ments were being sold for use in high school laboratories. Varian Optical Spectroscopy Instru ments contributed the Cary Model 11 UV-vis spectrophotometer, which was introduced in 1947. Howard Cary devel oped the automatic recording photoelec tric spectrophotometer for UV-vis regions using a double-prism monochromator to obtain high dispersion and freedom from scattered radiation. Wyatt Technology has loaned the Dif ferential I light-scattering photometer manufactured by Science Spectrum in 1970. This instrument was thefirstcom mercially produced light-scattering pho tometer that incorporated a laser light source. Its intended purpose was the de termination of molecular weights by clas sical light-scattering techniques, and it was also used by many researchers to study colloidal suspensions and other par ticulate characteristics by light scattering. Other instruments and equipment scheduled to be exhibited in the IR/UVvis area include a Michelson ruling en gine, a prism, holographic gratings with the Pittcon logo, a spectropolarimeter loaned by Carl Djerassi of Stanford Uni versity, and the flame photometer built by American Cyanamid and recognized as the precursor of the commercial instru ment developed by Perkin Elmer.
Antiquities Display Museum Exhibits Contributor
Instrument/Equipment
Section
Aerograph Model A-90 gas chromatograph Aerograph Model 600D HyFi gas chromatograph Aerograph Model 4010-01 liquid chromatograph Amino-Bowman spectrofluorometer Analytical Chemistry retrospective ARL production control quantometer (PCQ) Assayer's balance Bausch & Lomb Spectronic 20 Beckman IR-1 infrared spectrophotometer Beckman Model Β spectrophotometer Beckman Model DU UV-vis spectrophotometer Beckman Model G pH meter Blender Model Β Buchler rotoevaporator Cahn Model M-10 microbalance Carlo Erba Fractovap Model Gl Cary Model 11 UV-vis spectrophotometer Catalog #1250 ultraspeed electroanalyzer Catalog #1510 Dyna-Cath Catalog of early products Cells and accessories Cianflone Portaspec Coulter Model A DigiSorb 2500 surface area analyzer Dionex Model 10 ion chromatograph DuPont Model 900 thermal analyzer Early AA precursor instruments EDAX ECON detector EDAX Model 707 analyzer Evelyn photoelectric colorimeter (Rubicon) F&M Scientific Model 402 gas chromatograph F&M Scientific Model 700 gas chromatograph F&M Scientific Model 720 gas chromatograph F&M Scientific Model 810 gas chromatograph F-04 cell Fisher electrophotometer Flame photometer Fluoride ion selective electrode Frustrated reflection fingerprinting Gratings Harvard trip balance Heating mantle History of the American Society for Mass Spectrometry History of the MS-9 mass spectrometer History of the 103 C mass spectrometer Holographic gratings HP Model 1082 supercritical fluid chromatograph HP Model 5950 X-ray photoelectron spectrometer HP Model 5992 GC/MS instrument Hupe and Busch Model 1010 liquid chromatograph Hupe and Busch Model 1045 glass drawing machine Internal Reflection Spectroscopy Isco Dialagrad LC pump
Varian Chromatography Systems Chromatography Chromatography Varian Chromatography Systems Varian Chromatography Systems Chromatography IR/UV-vis spectroscopies Milton Roy 1950s Laboratory Analytical Chemistry/ACS Fisons Instruments Atomic spectroscopy Denver Instrument Company Balances IR/UV-vis spectroscopies Milton Roy IR/UV-vis spectroscopies Beckman Instruments 1950s Laboratory Beckman Instruments Beckman Instruments IR/UV-vis spectroscopies 1950s Laboratory Beckman Instruments 1950s Laboratory Waring Products 1950s Laboratory Labconco ATI Orion Research Balances Chromatography Fisons Instruments Varian Optical Spectroscopy IR/UV-vis spectroscopies 1950s Laboratory Eberbach 1950s Laboratory Eberbach IR/UV-vis spectroscopies Graseby Specac Beckman Instruments IR/UV-vis spectroscopies Cianflone Scientific Instruments X-ray spectrometers Particle size/surface area/pore size instruments Coulter Particle size/surface area/pore size instruments Micromeritics Chromatography Dionex TA Instruments Thermal equipment Alan Walsh Atomic spectroscopy EDAX International X-ray spectrometers EDAX International X-ray spectrometers G. L. Carlson IR/UV-vis spectroscopies Chromatography Hewlett Packard Chromatography Hewlett Packard Chromatography Hewlett Packard Chromatography Hewlett Packard Graseby Specac IR/UV-vis spectroscopies 1950s Laboratory Fisher Scientific IR/UV-vis spectroscopies American Cyanamid ATI Orion Research 1950s Laboratory Harrick Scientific IR/UV-vis spectroscopies Atomic spectroscopy Hitachi Balances Ohaus Corporation 1950s Laboratory Glas-Col M. A. Grayson Mass spectrometers M. A, Grayson Mass spectrometers Mass spectrometers M. A. Grayson Foil Miller IR/UV-vis spectroscopies Chromatography Hewlett Packard University of Pittsburgh Surface analyzers Hewlett Packard Mass spectrometers Chromatography Hewlett Packard Chromatography Hewlett Packard Harrick Scientific IR/UV-vis spectroscopies Chromatography Isco
Analytical Chemistry, Vol. 66, No. 4, February 15, 1994 221 A
GUIDE
Antiquities Display Museum Exhibits (Continued) Instrument/Equipment
Section
Isco Model U LC UV detector Jarrell Ash 21-ft. Wadsworth spectrograph JCPDS search/match cards Kipp hydrogen gas generator Laboratory Equipment display Lee Scientific Model 501 supercritical fluid chromatograph Metrohm Titrator Model 336 Mettler B5 balance Michelson ruling engine Micro-Tek Model 222 gas chromatograph Model 801 digital pH meter NaCI plates, demountable cells, and KBr die Norelco Powder Diffractometer Model 2 Numinco Orr surface analyzer Original ICP stand from ARL ICP-AES PAR Model 174 polarographic analyzer Parafilm PE DSC 1 differential scanning calorimeter PE Model 12 single-beam IR spectrophotometer PE Model 21 IR spectrophotometer PE Model 137 IR spectrophotometer PE Model 154 vapor fractometer PE Model 226 gas chromatograph PE Model 303 AA spectrophotometer PE Model 800 gas chromatograph pH meters, glass, and hot plate Photomultuplier tubes Physical Electronics Industries Model 10-150 Auger analyzer Prism liquid cell Prism Pye Argon gas chromatograph SediGraph 5000 automatic particle analyzer Separation Sciences Differential I light-scattering photometer Spectropolarimeter 3-Meter grating spectrograph 3M Model 520 ion scattering spectrometer 3M Combined ISS/SIMS system Tracor Model C321 Coulson conductivity detector Type Τ analytical balance Type FDM microbalance Type BB analytical balance Ultra Carbon carbon electrodes Variable cell Varian Model A-60 NMR spectrometer Waters Model 401 refractometer Waters Pico-Tag amino acid analysis system Waters Model U6K injector Waters Model 6000 LC pump Waters GPC Model 100 gel permeation chromatograph Zymate I Controller Zymate I Laboratory Automation System
Chromatography Isco Atomic spectroscopy Thermo Jarrell Ash ICDD X-ray spectrometers 1950s Laboratory Kipp and Zonen 1950s Laboratory Gordon Publications Chromatography Dionex 1950s Laboratory Brinkman Instruments Mettler-Toledo Balances IR/UV-vis spectroscopies Foil Miller Chromatography Tremetrics 1950s Laboratory ATI Orion Research Perkin Elmer IR/UV-vis spectroscopies X-ray spectrometers Phillips Electronic Instrument Particle size/surface area/pore size instruments Micromeritics Atomic spectroscopy Fisons Instruments Polarography EG&G Instruments 1950s Laboratory American National Can Perkin Elmer Thermal equipment IR/UV-vis spectroscopies Perkin Elmer Perkin Elmer IR/UV-vis spectroscopies Perkin Elmer IR/UV-vis spectroscopies Perkin Elmer Chromatography Chromatography Perkin Elmer Perkin Elmer Atomic spectroscopy Chromatography Perkin Elmer 1950s Laboratory Corning Atomic spectroscopy Hamamatsu
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Contributor
Surface analyzer IR/UV-vis spectroscopies IR/UV-vis spectroscopies Chromatography Particle size/surface area/pore size instruments
Perkin Elmer Harrick Scientific Foil Miller ATI Orion Research Micromeritics
IR/UV-vis spectroscopies IR/UV-vis spectroscopies Atomic spectroscopy Surface analyzers Surface analyzers Chromatography Balances Balances Balances 1950s Laboratory IR/UV-vis spectroscopies NMR Chromatography Chromatography Chromatography Chromatography Chromatography Autoanalyzers Autoanalyzers
Wyatt Technology Carl Djerassi Baird Analytical Advanced R&D Advanced R&D Tremetrics Denver Instrument Company Denver Instrument Company Denver Instrument Company Carbone of America Graseby Specac PPG Industries Millipore Waters Millipore Waters Millipore Waters Millipore Waters Millipore Waters Zymark Zymark
Analytical Chemistry, Vol. 66, No. 4, February 15, 1994
